CN108118194B - Preparation method of Fe-Co-based magnetostrictive alloy wire - Google Patents

Abstract

The invention discloses a preparation method of Fe-Co-based magnetostrictive alloy wire, which comprises the following steps: putting ingredients into a vacuum induction furnace, introducing argon gas to protect them for smelting, and casting into cylindrical Fe-Co after smelting Alloy ingots; Fe-Co alloy ingots are heated and kept warm and then forged into Fe-Co alloy round bars, Fe-Co alloy round bars are hot rolled into Fe-Co alloy wire rods, and Fe-Co alloy wire rods are hot drawn into Fe-Co alloy wire rods. Fe-Co alloy wire, surface-treated Fe-Co alloy wire, and cold drawn into Fe-Co-based magnetostrictive wire; Fe-Co-based magnetostrictive wire is heat-treated at 700-900℃ in a vacuum heating furnace, and kept at For 0.5-1 hour, use water quenching or air cooling to cool to room temperature. The invention solves the problem of unstable magnetic properties and mechanical properties of the existing magnetostrictive alloy wire.

Description

Preparation method of Fe-Co-based magnetostrictive alloy wire

technical field

The invention relates to a magnetostrictive material, in particular to a preparation method of Fe-Co-based magnetostrictive alloy wire.

Background technique

Magnetostrictive materials have the characteristics of recovering deformation in the presence of an external magnetic field and changing magnetic properties when stress is applied. They are important functional materials for energy and information conversion. At present, there are four main types of magnetostrictive materials used in engineering: First, metals and alloys with magnetostrictive effect, such as nickel-based alloys and iron-based alloys, have high saturation magnetization, good mechanical properties, and can be The characteristics of deformation; the second is ferrite (such as Ni-Zn, Ni-Co-Cu, etc.), which has low saturation magnetization, low price, and good high-frequency characteristics; the third is rare earth represented by Tb-Dy-Fe materials Intermetallic compounds, their magnetostrictive properties are much higher than traditional magnetostrictive materials, but they are brittle, cannot be processed into silk, and the raw materials are expensive; the fourth is Fe-Ga giant magnetostrictive materials, which have better magnetostrictive properties. Stretching and mechanical properties.

As a smart material, magnetostrictive materials are widely used in technical fields such as energy conversion, driving, and sensing. The liquid level sensor developed by the Wiedemann effect of magnetostrictive materials has a wide range of applications in modern industry. Most of the waveguide wires of the core sensitive components are Fe-Ni alloy wires, but the magnetostrictive properties of Fe-Ni alloy wires are low, which limits the accuracy and measurement range of the sensor. Therefore, a magnetostrictive alloy wire with a simple preparation process and both large magnetostriction and good mechanical properties has become the focus of attention.

SUMMARY OF THE INVENTION

The technical problem solved by the present invention is to provide a preparation method of Fe-Co-based magnetostrictive alloy wire, which solves the problem of unstable magnetic and mechanical properties of the existing magnetostrictive alloy wire.

The technical solution is as follows:

A Fe-Co-based magnetostrictive alloy, characterized in that: the weight percentage of the alloy composition is Fe _{100-xy- z Co x} My RE _z , and M is one of Mn, V, Cu, Ti, and Al or Multiple, RE is one or more of La, Ce, Pr, Tb, Dy, Y, Er, wherein x=60-80, y=0-10, z=0.1-1.0, and the balance is Fe.

Further: x=65-75, y=0, z=0.1-1.0, and the remainder is Fe.

Further: x=65-75, y=0-5, and 65≤x+y≤80, z=0.1-1.0, and the remainder is Fe.

A preparation method of Fe-Co-based magnetostrictive alloy wire, comprising:

According to the mass percentage of the alloy composition, the ingredients are added, and an appropriate amount of burning loss is added; the ingredients are put into a vacuum induction furnace, evacuated to 5-10Pa, and smelted under argon protection. Co alloy ingot; the weight percentage of alloy composition is Fe _100-xyz Co _{x My} RE _z , M is one or more of Mn, V, Cu, Ti, Al, RE is La, Ce, Pr, Tb One or more of , Dy, Y, Er, wherein x=60-80, y=0-10, z=0.1-1.0, and the remainder is Fe;

The Fe-Co alloy ingot is heated to 600-900°C, and then forged after being kept for 1-3 hours, and finally forged to a Fe-Co alloy round bar with a diameter of 30-35mm;

The Fe-Co alloy round bar is heated to 800-1000 ℃ for hot rolling, wherein the total rolling passes are 7-10 times, and the Fe-Co alloy wire rod with a diameter of 7.0-8.0mm is prepared;

The Fe-Co alloy wire rod is heated to 800-1000°C for hot drawing, wherein the total drawing passes are 8-10 times, and Fe-Co alloy wire with a diameter of 2.5-3.5mm is prepared;

The Fe-Co alloy wire is surface-treated and cold drawn, wherein the total drawing passes are 20-25 times, and the Fe-Co-based magnetostrictive wire with a diameter of 0.5-1.0 mm is used;

The Fe-Co-based magnetostrictive wire is heat-treated at 700-900° C. in a vacuum heating furnace, kept for 0.5-1 hour, and cooled to room temperature by water quenching or air cooling.

Preferably: the surface of the Fe-Co alloy ingot is ground to remove the surface oxide layer and defects.

Preferably: during the forging process, the final forging temperature is controlled to not be lower than 500°C, the forging is terminated when the temperature is lower than 500°C, and the forging is continued after returning to the furnace for 10-30 minutes.

Preferably: after the forging is completed, the surface of the Fe-Co alloy round bar is ground to remove the surface oxide layer and defects of the Fe-Co alloy round bar.

Preferably: during the hot rolling process, the final rolling temperature is controlled to not be lower than 700°C, the hot rolling is terminated when the temperature is lower than 700°C, and the hot rolling is continued after being kept in the furnace for 10-20 minutes.

Preferably: pickling and alkaline washing are performed before hot drawing Fe-Co alloy wire rods, and after cold drawing is completed, Fe-Co alloy wire is subjected to pickling and alkaline washing to remove surface oxide layer.

Preferably: solution treatment is performed during the cold drawing process, the treatment temperature is 500-700° C., the treatment time is 1-3 hours, and the cooling method is water cooling or air cooling.

Compared with the prior art, the technical effects of the present invention include:

1. The present invention solves the problem of unstable magnetic properties and mechanical properties of the existing magnetostrictive alloy wires. The preparation process of Fe-Co magnetostrictive material is simple and easy, the magnetic and mechanical properties are stable, and the magnetostrictive coefficient reaches 80×10 ^-6 , which is nearly 5 times higher than that of the traditional iron-nickel alloy. , without negatively affecting other magnetic properties.

2. The present invention improves the toughness and tensile properties of the magnetostrictive wire by adding elements such as Mn, V, Cu, Ti, and Al, so that the diameter of the alloy wire reaches 0.5-1.0 mm.

3. The optimization and improvement of the preparation of Fe-Co alloy magnetostrictive wires reduces the preparation cost, and can improve the stability of material preparation, which is convenient for large-scale mass production. Further, the wide application of Fe-Co alloy magnetostrictive alloy wires in sensors is realized.

Description of drawings

Fig. 1 is the magnetostrictive performance curve diagram of Fe _26.5 Co ₇₃ Y _0.5 magnetostrictive alloy wire in the present invention;

Fig. 2 is the magnetostrictive performance curve diagram of Fe ₂₀ Co ₇₉ Mn _0.8 Tb _0.2 magnetostrictive alloy wire in the present invention;

Fig. 3 is a graph showing the magnetostrictive performance of the Fe _23.2 Co ₇₆ Cu _0.5 Ce _0.3 magnetostrictive alloy wire in the present invention.

Detailed ways

The technical solutions of the present invention will be described in detail below with reference to the exemplary embodiments. Example embodiments, however, can be embodied in various forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art.

The preparation method of Fe-Co-based magnetostrictive alloy wire is prepared by hot drawing method, and the details are as follows:

Step 1: Make ingredients according to the mass percentage of alloy components, and add an appropriate amount of burning loss; put the ingredients into a vacuum induction furnace, evacuate to 5-10Pa, pass argon protection for smelting, and cast into a cylinder after smelting Shaped Fe-Co alloy ingot;

Fe-Co-based magnetostrictive alloy, the weight percentage of the alloy composition is: Fe _100-xyz Co _{x My} RE _z , M is one or more of Mn, V, Cu, Ti, Al, RE is La, One or more of Ce, Pr, Tb, Dy, Y, Er, wherein x=60-80, y=0-10, z=0.1-1.0, and the balance is Fe.

The surface of the Fe-Co alloy ingot is ground to remove the surface oxide layer and defects, and finally the Fe-Co alloy ingot with a smooth surface is obtained.

Step 2: heating the Fe-Co alloy ingot to 600-900°C, forging after 1-3 hours of heat preservation, and finally forging to a Fe-Co alloy round bar with a diameter of 30-35mm;

Control the final forging temperature not lower than 500 ℃, stop forging when it is lower than 500 ℃, and continue forging after returning to the furnace for 10-30 minutes. After the forging is completed, the surface of the Fe-Co alloy round rod is ground to remove the surface oxide layer and defects of the Fe-Co alloy round rod, and finally a Fe-Co alloy round rod with a smooth surface is obtained.

Step 3: Heating the Fe-Co alloy round bar to 800-1000°C, and using a four-roll mill for hot rolling, wherein the total number of rolling passes is 7-10 times, to prepare Fe-Co with a diameter of 7.0-8.0mm alloy wire rod;

It is necessary to control the final rolling temperature not to be lower than 700 ℃, stop the hot rolling when it is lower than 700 ℃, and continue the hot rolling after returning to the furnace for 10-20 minutes.

Step 4: heating the Fe-Co alloy wire rod to 800-1000°C, and using a horizontal wire drawing machine for hot drawing, wherein the total drawing passes are 8-10 times to prepare Fe- Co alloy wire;

Before hot drawing Fe-Co alloy wire rods, pickling and alkali washing are carried out to remove the surface oxide layer.

Step 5: The Fe-Co alloy wire is surface-treated and cold drawn by a horizontal wire drawing machine, wherein the total drawing passes are 20-25 times, and the Fe-Co-based magnetostrictive wire with a diameter of 0.5-1.0 mm is used;

After the cold drawing is completed, the Fe-Co alloy wire is subjected to pickling and alkali washing treatment to remove the surface oxide layer. In the process of cold drawing, solution treatment is required, the treatment temperature is 500-700 ℃, the treatment time is 1-3 hours, and the cooling method is water cooling or air cooling.

Step 6: The Fe-Co-based magnetostrictive wire is heat-treated at 700-900° C. in a vacuum heating furnace, kept for 0.5-1 hour, and cooled to room temperature by water quenching or air cooling to obtain Fe-Co-based magnetostrictive alloy wire .

The purity of the selected raw materials in the examples of the present invention are all above 99.95%. In the embodiment of the present invention, the magnetostrictive strain is measured in the parallel direction by using the standard resistance strain gauge method.

The technical solutions of the present invention will be further described in detail below through the examples.

Example 1:

Step 1: Weigh the raw materials of Fe 26.5%, Co 73%, Y 0.5% according to the weight percentages, the sum of the weight percentages of the above components is 100%, put the raw materials into the vacuum induction furnace, vacuumize to 8Pa, pass through It is smelted under argon protection and cast into cylindrical ingots after smelting; then the surface of the alloy is polished to remove the surface oxide layer and defects of the Fe-Co alloy ingot, and finally a smooth surface Fe-Co alloy ingot is obtained ;

Step 2: Heat the Fe-Co alloy ingot to 850°C, hold it for 1 hour before forging, the final forging temperature is 700°C, and finally forge to an alloy round bar with a diameter of 31mm, which needs to be controlled during this process, when the temperature is lower than 700°C The forging was terminated, and the forging was continued after returning to the furnace for 20 minutes. After the forging was completed, the surface of the alloy was ground to remove the surface oxide layer and defects of the Fe-Co alloy rod, and finally a Fe-Co alloy round rod with a smooth surface was obtained;

Step 3: Heat the Fe-Co alloy round bar to 1000°C, use a four-roll mill for hot rolling, control the final rolling temperature to 900°C, stop hot rolling when it is lower than 900°C, and continue hot rolling after 15 minutes of heat preservation. Pass rolling to prepare Fe-Co alloy wire rods with a diameter of 8.0 mm;

Step 4: The Fe-Co alloy wire rod is subjected to acid washing and alkali washing treatment, the surface oxide layer is removed, and then heated to 1000 ° C, and the horizontal wire drawing machine is used for hot drawing. Fe-Co based magnetostrictive wire;

Step 5: The Fe-Co alloy wire is surface-treated, and the horizontal wire drawing machine is used for cold drawing, and the total drawing passes is 20 times to prepare Fe-Co-based magnetostrictive wires with a diameter of 0.8 mm. Carry out solution treatment, the treatment temperature is 700 ℃, the treatment time is 1.5 hours, and the cooling method is water cooling;

Step 6: The Fe-Co-based magnetostrictive wire is heat-treated at 800° C. in a vacuum heating furnace, kept for 0.5 hours, and cooled to room temperature by water quenching to obtain the Fe-Co-based magnetostrictive alloy wire.

As shown in FIG. 1 , it is a graph of the magnetostrictive performance of the Fe _26.5 Co ₇₃ Y _0.5 magnetostrictive alloy wire in the present invention.

When the magnetic field is 2000Oe, the magnetostriction coefficient reaches 76×10 ^-6 ; when the magnetic field is 4000Oe, the magnetostriction reaches saturation, and the coefficient is 81×10 ^-6 .

Example 2:

Step 1: Weigh the raw materials of Fe 20%, Co 79%, Mn 0.8%, Tb 0.2% according to the weight percentage, the sum of the weight percentages of the above components is 100%, put the raw materials into the vacuum induction furnace, Vacuuming to 10Pa, smelting with argon protection, and casting into cylindrical ingots after smelting; then grinding the surface of the alloy to remove the surface oxide layer and defects of the Fe-Co alloy ingot, and finally obtain a smooth surface. Fe-Co alloy ingot;

Step 2: Heat the Fe-Co alloy ingot to 700°C, hold it for 1.5 hours before forging, the final forging temperature is 600°C, and finally forge to an alloy round bar with a diameter of 35mm, which needs to be controlled during this process, when the temperature is lower than 600°C The forging was terminated, and the forging was continued after returning to the furnace for 15 minutes; after the forging was completed, the surface of the alloy was ground to remove the surface oxide layer and defects of the Fe-Co alloy rod, and finally a smooth surface Fe-Co alloy rod was obtained;

Step 3: Heat the Fe-Co alloy round bar to 900°C, use a four-roll mill for hot rolling, control the final rolling temperature to 700°C, stop hot rolling when it is lower than 700°C, and continue hot rolling after returning to the furnace for 20 minutes of heat preservation. Pass rolling to prepare Fe-Co alloy wire rods with a diameter of 7.5mm;

Step 4: The Fe-Co alloy wire rod is subjected to acid washing and alkali washing treatment, and the surface oxide layer is removed, and then heated to 900 ° C, and the horizontal wire drawing machine is used for hot drawing. Fe-Co based magnetostrictive wire;

Step 5: The Fe-Co alloy wire is surface-treated, and the horizontal wire drawing machine is used for cold drawing, and the total drawing passes is 23 times to prepare Fe-Co-based magnetostrictive wires with a diameter of 0.6 mm. Carry out solution treatment, the treatment temperature is 700 ℃, the treatment time is 1 hour, and the cooling method is air cooling;

Step 6: The Fe-Co-based magnetostrictive wire is heat-treated at 900° C. in a vacuum heating furnace, kept for 1 hour, and cooled to room temperature by air cooling to obtain the Fe-Co-based magnetostrictive alloy wire.

As shown in FIG. 2 , it is a graph of the magnetostrictive performance of the Fe ₂₀ Co ₇₉ Mn _0.8 Tb _0.2 magnetostrictive alloy wire in the present invention.

When the magnetic field is 2000Oe, the magnetostriction coefficient reaches 78×10 ^-6 ; when the magnetic field is 4000Oe, the magnetic extension reaches saturation, and the coefficient is 80×10 ^-6 .

Example 3:

Step 1: Weigh the raw materials of Fe 23.2%, Co 76%, Cu 0.5%, Ce 0.3% according to the weight percentages, the sum of the weight percentages of the above components is 100%, put the raw materials into the vacuum induction furnace, and extract the raw materials. Vacuum to 10Pa, pass argon protection for smelting, and cast into cylindrical ingots after smelting; then grind the surface of the alloy to remove the surface oxide layer and defects of the Fe-Co alloy ingot, and finally obtain a smooth surface Fe -Co alloy ingots;

Step 2: Heating the Fe-Co alloy ingot to 800°C, holding it for 2 hours, then forging, the final forging temperature is 600°C, and finally forging to an alloy round bar with a diameter of 35mm, which needs to be controlled during this process, when the temperature is lower than 600°C The forging was terminated, and the forging was continued after returning to the furnace for 10 minutes. After the forging was completed, the surface of the alloy was ground to remove the surface oxide layer and defects of the Fe-Co alloy rod, and finally a Fe-Co alloy round rod with a smooth surface was obtained;

Step 3: Heat the Fe-Co alloy round bar to 900°C, use a four-high rolling mill for hot rolling, control the final rolling temperature to 700°C, stop the hot rolling when it is lower than 700°C, and continue the hot rolling after returning to the furnace for 20 minutes. Pass rolling to prepare Fe-Co alloy wire rods with a diameter of 7.0mm;

Step 4: The Fe-Co alloy wire rod is subjected to acid washing and alkali washing treatment, and the surface oxide layer is removed, and then heated to 900 ° C, and the horizontal wire drawing machine is used for hot drawing. Fe-Co based magnetostrictive wire;

Step 5: The Fe-Co alloy wire is surface-treated, and the horizontal wire drawing machine is used for cold drawing, and the total drawing passes is 25 times to prepare Fe-Co-based magnetostrictive wires with a diameter of 0.5 mm. Carry out solution treatment, the treatment temperature is 650 ° C, the treatment time is 2 hours, and the cooling method is water cooling;

Step 6: The Fe-Co-based magnetostrictive wire is heat-treated at 900° C. in a vacuum heating furnace, kept for 1 hour, and cooled to room temperature by air cooling to obtain the Fe-Co-based magnetostrictive alloy wire.

As shown in FIG. 3 , it is a graph showing the magnetostrictive performance of the Fe _23.2 Co ₇₆ Cu _0.5 Ce _0.3 magnetostrictive alloy wire in the present invention.

When the magnetic field is 2000Oe, the magnetostriction coefficient reaches 75×10 ^-6 ; when the magnetic field is 3500Oe, the magnetostriction reaches saturation, and the coefficient is 80×10 ^-6 .

The terms used in the present invention are terms of description and illustration, not limitation. Since the invention can be embodied in many forms without departing from the spirit or essence of the invention, it is to be understood that the above-described embodiments are not limited to any of the foregoing details, but are to be construed broadly within the spirit and scope defined by the appended claims Therefore, all changes and modifications that come within the scope of the claims or their equivalents should be covered by the appended claims.

Claims (6)

1. A preparation method of Fe-Co-based magnetostrictive alloy wires comprises the following steps:

mixing the materials according to the mass percentage of the alloy components, and adding a proper amount of burning loss; putting the ingredients into a vacuum induction furnace, vacuumizing to 5-10Pa, introducing argon for protection to carry out smelting, and casting into a cylindrical Fe-Co alloy ingot after the smelting is finished; the weight percentage of the alloy component is Fe_100-x-y-zCo_xM_yRE_zM is one or more of Mn, V, Cu, Ti and Al, RE is one or more of La, Ce, Pr, Tb, Dy, Y and Er, wherein x is 60-80, Y is 0-10, z is 0.1-1.0, and the balance is Fe;

heating the Fe-Co alloy ingot to 600-;

heating the Fe-Co alloy round bar to 800-1000 ℃ for hot rolling, wherein the total rolling pass is 7-10 times, and preparing the Fe-Co alloy wire rod with the diameter of 7.0-8.0 mm;

heating the Fe-Co alloy wire rod to 800-;

carrying out surface treatment on the Fe-Co alloy wire, and carrying out cold drawing, wherein the total drawing passes are 20-25 times, and the diameter of the Fe-Co-based magnetostrictive wire is 0.5-1.0 mm;

the Fe-Co-based magnetostrictive wire is subjected to heat treatment at the temperature of 700-900 ℃ in a vacuum heating furnace, is kept for 0.5-1 hour, and is cooled to the room temperature by water quenching or air cooling.

2. The method for producing an Fe-Co-based magnetostrictive alloy wire according to claim 1, characterized in that: in the forging process, the final forging temperature is controlled to be not lower than 500 ℃, the forging is stopped when the temperature is lower than 500 ℃, and the forging is continued after the furnace is returned and the temperature is preserved for 10 to 30 minutes.

3. The method for producing an Fe-Co-based magnetostrictive alloy wire according to claim 1 or 2, characterized in that: and polishing the surface of the Fe-Co alloy cast ingot, polishing the surface of the Fe-Co alloy round rod after forging is completed, and removing a surface oxidation layer and defects of the Fe-Co alloy round rod.

4. The method for producing an Fe-Co-based magnetostrictive alloy wire according to claim 1 or 2, characterized in that: and in the hot rolling process, controlling the final rolling temperature to be not lower than 700 ℃, stopping hot rolling when the final rolling temperature is lower than 700 ℃, returning to the furnace and keeping the temperature for 10-20 minutes, and then continuing hot rolling.

5. The method for producing an Fe-Co-based magnetostrictive alloy wire according to claim 1, characterized in that: and carrying out acid washing and alkali washing treatment before hot drawing the Fe-Co alloy wire rod, and carrying out acid washing and alkali washing treatment on the Fe-Co alloy wire after cold drawing is finished to remove a surface oxide layer.

6. The method for producing an Fe-Co-based magnetostrictive alloy wire according to claim 1, characterized in that: the solution treatment is carried out in the cold drawing process, the treatment temperature is 500-700 ℃, the treatment time is 1-3 hours, and the cooling mode is water cooling or air cooling.

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